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Method for detecting content of sodium thiosulfate in sodium hexamethylene-1,6-bisthiosulfate dehydrate

A technology of disodium dithiosulfate and hexamethylene dihydrate, which is applied in the field of impurity detection, can solve problems affecting the accuracy of detection results, and achieve the effect of being suitable for large-scale application, accurate detection results, and simple operation

Inactive Publication Date: 2019-09-06
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the iodometric method has the advantages of simple operation and low cost, it can be seen from the HTS structural formula that HTS itself has a sulfite structure, which can react with elemental iodine, so if the iodometric method is directly used for determination, it will definitely affect Accuracy of test results

Method used

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  • Method for detecting content of sodium thiosulfate in sodium hexamethylene-1,6-bisthiosulfate dehydrate
  • Method for detecting content of sodium thiosulfate in sodium hexamethylene-1,6-bisthiosulfate dehydrate
  • Method for detecting content of sodium thiosulfate in sodium hexamethylene-1,6-bisthiosulfate dehydrate

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Effect test

Embodiment 1

[0048] The detection method of sodium thiosulfate content in the dihydrate hexamethylene-1,6-dithiosulfate disodium salt provided by the present invention is used to measure the sodium thiosulfate solution of known concentration (in this solution Add a certain quality of sodium chloride standard substance), to verify the detection method of the present invention, the steps are as follows:

[0049] Step 1: Solution configuration and calibration:

[0050] Ferric ammonium sulfate indicator: Dissolve about 5g of ferric ammonium sulfate dodecahydrate in 50ml of distilled water with a little nitric acid added dropwise.

[0051] Dilute nitric acid solution: Mix concentrated nitric acid and distilled water at a volume ratio of 1:3.

[0052] Preparation and calibration of silver nitrate solution:

[0053] Preparation: Accurately weigh 8.50g of silver nitrate, dissolve it in distilled water, and use a 500ml brown volumetric flask for constant volume to obtain a silver nitrate solution...

Embodiment 2

[0085] Determination of the content of sodium thiosulfate in unknown HTS products, the steps are as follows:

[0086] Step 1 is the same as the step in Example 1; prepare dilute nitric acid solution, 0.1mol / L silver nitrate solution, 0.025mol / L ammonium thiocyanate obtained by ferric ammonium sulfate indicator, concentrated nitric acid and distilled water with a volume ratio of 1:3 solution;

[0087] Step 2: Determination of chloride content (calculated as sodium chloride): add 0.2010g HTS sample and 30ml ultrapure aqueous solution in 100ml Erlenmeyer flask, first add 10ml dilute nitric acid solution (10%), add 5ml 0.1mol / L Silver nitrate solution (if there is a small amount of sodium thiosulfate remaining in the sample, the solution will turn orange-red or black precipitate will appear). Slowly heat the solution to be tested until the solution turns from cloudy to transparent and colorless, with a small amount of white precipitate at the bottom. After the solution is cooled...

Embodiment 3

[0103] Weigh 0.2217g of the HTS sample in Example 2 and mix it with a sodium thiosulfate solution with a known content of 0.004g as the sample to be tested. The relationship between the measured value and the theoretical value is compared, so as to further verify the accuracy of the test method of the present invention.

[0104] Step 1 is the same as the step in Example 1; prepare dilute nitric acid solution, 0.1mol / L silver nitrate solution, 0.025mol / L ammonium thiocyanate obtained by ferric ammonium sulfate indicator, concentrated nitric acid and distilled water with a volume ratio of 1:3 solution;

[0105] Step 2: Determination of chloride content (in sodium chloride): 0.2257g of the sample to be tested is dissolved in 10ml of water, first add 10ml of nitric acid solution (10%), add 5ml of 0.1mol / L silver nitrate solution (if in the sample There is a small amount of sodium thiosulfate remaining, the solution will turn orange-red or a black precipitate will appear). Slowly...

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Abstract

The invention provides a method for detecting the content of sodium thiosulfate in the sodium hexamethylene-1,6-bisthiosulfate dehydrate. A chloride ion content of a to-be-detected HTS sample is measured to avoid the influence on a detection result by chloride ions. When the to-be-detected sample is preprocessed, excessive silver nitrate solution and dilute nitric acid are added; and the dilute nitric acid decomposes sodium thiosulfate in the sample and thus the silver nitrate only reacts with the chloride ion in the HTS. After interference component removing, the content of sodium thiosulfatein the sample can be accurately detected by a simple silver method. The method has advantages of simple preprocessing process, simple operation, and low cost; the interference component in the detection process of the iodometric method can be removed fully; the detection result is accurate; and the method is suitable for large-scale popularization and application.

Description

technical field [0001] The invention belongs to the technical field of impurity detection, in particular to a method for detecting sodium thiosulfate content in dihydrated hexamethylene-1,6-dithiosulfate disodium salt (HTS) products. Background technique [0002] Anti-reversion agent dihydrate hexamethylene-1,6-dithiosulfate disodium salt, hereinafter referred to as HTS, its chemical formula is C 6 h 12 Na 2 o 6 S 4 2H 2 O, the molar mass is 390.43. Its structural formula is as follows, and its own structure contains two sulfite groups: [0003] [0004] As a rubber additive, HTS is widely used in the rubber field, which greatly improves the thermal stability of rubber. Adding HTS to the natural rubber sulfenamide vulcanization system can produce thermally stable C-C crosslinks during the vulcanization process. C-C The cross-linking bond can compensate for the polysulfide bond lost due to vulcanization reversion and chain scission, and form a compound cross-linking...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N21/78G01N1/28
CPCG01N1/28G01N21/78G01N31/16
Inventor 黄存影张新凤李庆朝杜孟成师利龙王克军
Owner SHANDONG YANGGU HUATAI CHEM
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